JP2007521392A - 多層膜高温超伝導(hts)コートテープを製造する有機金属気相成長(mocvd)プロセス、および装置 - Google Patents
多層膜高温超伝導(hts)コートテープを製造する有機金属気相成長(mocvd)プロセス、および装置 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000008569 process Effects 0.000 title claims description 22
- 229910052751 metal Inorganic materials 0.000 title description 5
- 239000002184 metal Substances 0.000 title description 5
- 238000005229 chemical vapour deposition Methods 0.000 title description 3
- 239000000758 substrate Substances 0.000 claims abstract description 127
- 238000000151 deposition Methods 0.000 claims abstract description 95
- 230000008021 deposition Effects 0.000 claims abstract description 91
- 239000006200 vaporizer Substances 0.000 claims abstract description 18
- 239000012705 liquid precursor Substances 0.000 claims abstract description 15
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract 7
- 239000002243 precursor Substances 0.000 claims description 208
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 43
- 239000001301 oxygen Substances 0.000 claims description 42
- 229910052760 oxygen Inorganic materials 0.000 claims description 42
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 claims description 40
- IQAKAOAPBMJSGJ-UHFFFAOYSA-N [Cu].[Y].[Ba] Chemical compound [Cu].[Y].[Ba] IQAKAOAPBMJSGJ-UHFFFAOYSA-N 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 24
- 238000000576 coating method Methods 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000012691 Cu precursor Substances 0.000 claims description 8
- -1 SmBCO Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims description 2
- 230000008016 vaporization Effects 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 82
- 239000010408 film Substances 0.000 description 64
- 239000000463 material Substances 0.000 description 22
- 238000010438 heat treatment Methods 0.000 description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 239000012159 carrier gas Substances 0.000 description 14
- 239000007789 gas Substances 0.000 description 14
- HOPFUPXNYITIIP-UHFFFAOYSA-N [Cu].[Ba].[Sm] Chemical compound [Cu].[Ba].[Sm] HOPFUPXNYITIIP-UHFFFAOYSA-N 0.000 description 13
- 239000004020 conductor Substances 0.000 description 13
- 230000036961 partial effect Effects 0.000 description 12
- 239000010949 copper Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000005137 deposition process Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- 230000007547 defect Effects 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 7
- 229910052788 barium Inorganic materials 0.000 description 7
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 230000003746 surface roughness Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229910052727 yttrium Inorganic materials 0.000 description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 125000002524 organometallic group Chemical group 0.000 description 4
- 238000004549 pulsed laser deposition Methods 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 230000003213 activating effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 229910016006 MoSi Inorganic materials 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910000953 kanthal Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000005749 Copper compound Chemical group 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- LGVUVWSTEGWVKM-UHFFFAOYSA-N [Cu]=O.[Ba].[Sm] Chemical compound [Cu]=O.[Ba].[Sm] LGVUVWSTEGWVKM-UHFFFAOYSA-N 0.000 description 1
- BTGZYWWSOPEHMM-UHFFFAOYSA-N [O].[Cu].[Y].[Ba] Chemical compound [O].[Cu].[Y].[Ba] BTGZYWWSOPEHMM-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 229910001026 inconel Inorganic materials 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910002076 stabilized zirconia Inorganic materials 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
Description
堆積温度:HTS膜の表面粗さは、堆積温度により影響される;
前駆体組成:たとえば、前駆体のモル濃度(濃度)は、該膜のモルフォロジーに影響を与える、たとえば、バリウム欠陥膜は、バリウムのリッチな膜ばかりでなく、化学量論膜とも異なるモルフォロジーをもつ;
前駆体供給レート:たとえば、堆積された最初の膜は、それが堆積ゾーン118を通るときに、連続的に高温にさらされ、これは、それが全体の堆積ゾーン118を通って移動しようとするとき、この最初の層のモルフォロジーに対してダメージを与える原因となる。続く層に対して、前駆体供給レートを増大することは、該最初の層が、この高加熱を経験する時間を短くし、かつ、これにより、ありうるダメージを最小化することができる。
酸素分圧:異なる酸素分圧および基板温度の下で膜を準備することが必要である。たとえば、前駆体供給レートが、0.25から0.5ml/min に2倍に増大したところでは、0.5Torr のより高い酸素分圧が持ちられるとき、よい性能が得られる。酸素分圧は、基板温度が増大したとき、上記例にしたがって、増大するであろう。酸素分圧は、処理パラメータの変化、たとえば、多区画シャワーヘッド112と基板テープ116との間の距離、UV光のソース蒸気への露出、または、原子酸素、またはオゾンの酸化剤としての使用、等、に依存して、実験的に決定することができる。
0.25ML/min の供給レート、および800℃の堆積温度を仮定して、前駆体の前駆体モル濃度(すなわち、溶液のリッターあたりの溶媒のモル数)の増加は、膜厚の増加を生ずる。たとえば、
0.030mol/L は、約1.0ミクロンの膜厚を生ずる。
0.045mol/L は、約1.25ミクロンの膜厚を生ずる。
0.060mol/L は、約1.75ミクロンの膜厚を生ずる。
0.30ML/min の前駆体モル濃度、および800℃の堆積温度を仮定して、前駆体の供給レートは、また、膜厚の増加を生ずる。たとえば、
0.25mL/min の供給レートは、約1.0ミクロンの膜厚を生ずる。
0.50mL/min の供給レートは、約2.0ミクロンの膜厚を生ずる。
1.00mL/min の供給レートは、約4.0ミクロンの膜厚を生ずる。
例1:0.03mol/L のモル濃度と結合して、0.56Torrの酸素分圧と結合した、0.25mL/min の供給レートは、0.6ミクロン厚の膜に対して、約2.7MA/cm2 の臨界電流を生じる(例1)。
例2:0.03mol/L のモル濃度と結合して、0.56Torrの酸素分圧と結合した、0.50mL/min の供給レートは、0.6ミクロン厚の膜に対して、約0.0A/cm2 の臨界電流を生じる(堆積時間が例1の半分に減少したとしても、同じ膜厚が得られる。)。
例3:0.03mol/L のモル濃度と結合して、1.08Torrの酸素分圧と結合した、0.50mL/min の供給レートは、0.6ミクロン厚の膜に対して、約2.5MA/cm2 の臨界電流を生じる(堆積時間が例1の半分に減少したとしても、同じ膜厚が得られる。)。
例4:0.06mol/L のモル濃度と結合して、1.08Torrの酸素分圧と結合した、0.50mL/min の供給レート、は、0.6ミクロン厚の膜に対して、約2.2MA/cm2 の臨界電流を生じる(堆積時間が例3の半分に減少したとしても、同じ膜厚が得られる。)。
基板ヒータ114内に、直接に区画113に関係付けられ、必要であれば、更なる温度制御のための堆積ゾーンを生じる分離されたヒータゾーンが設けられていてもよい。
Claims (22)
- 多層コートされた基板を製造するMOCVD堆積装置において、
真空チャンバーと、
ヒータと、
多区画シャワーヘッドと、少なくとも2つの1区画シャワーヘッドとからなるグループのうちから選択されたシャワーヘッド供給装置と、
少なくとも1つの前駆体駆動システムと、
基板移動システムと、を備え、
前記シャワーヘッドと前記ヒータとの間の空間は、コーティングの連続的な層が堆積される真空チャンバー内の延長された長さの堆積ゾーンを定義している、
ことを特徴とするMOCVD堆積装置。 - 請求項1の装置において、
前記多区画シャワーヘッドにおける2つ又はそれ以上の区画は、単一の前駆体供給システムに接続されている。 - 請求項1の装置において、
前記多区画シャワーヘッドにおける各区画は、単一の前駆体供給システムに接続されている。 - 請求項1の装置において、
少なくとも1つの前駆体供給システムは、液体前駆体のソース、ポンプ、不活性ガスのソース、前駆体蒸気化器、および酸素のソースからなる。 - 請求項1の装置において、
2つ、又はそれ以上の前駆体供給システムがあり、
その各々は、液体前駆体のソース、ポンプ、不活性ガスのソース、前駆体蒸気化器、および酸素のソースからなる。 - 請求項1の装置において、
前記多区画シャワーヘッドは、2つから7つの区画を持つ。 - 請求項1の装置において、
前記多区画シャワーヘッドは、5つの区画を持つ。 - 請求項7の装置において、
前記区画は、異なる供給長さを持つ。 - 請求項1の装置において、
前記ヒータは、マルチゾーンヒータを持つ。 - 請求項9の装置において、
前記ヒータは、多区画シャワーヘッドの各区画に対して1つのゾーンを含む。 - 多層コートされた基板を製造するプロセスであって、
真空チャンバーと、ヒータと、多区画シャワーヘッドと少なくとも2つの1区画を有するシャワーヘッドとからなるグループのうちから選択されたシャワーヘッド供給装置と、少なくとも1つの前駆体駆動システムと、基板移動システムと、を備え、前記シャワーヘッドと前記ヒータとの間の空間は、コーティングの連続的な層が堆積される真空チャンバー内の延長された長さの堆積ゾーンを定義しているMOCVDチャンバーによってコートされるべき基板を移動させることよりなり、かつ、
前記延長された長さの堆積ゾーンを通る基板は、前記ヒータにより加熱され、前記個々のシャワーヘッド区画の各々に存在する蒸気化された前駆体を連続的に照射されてその上にコーティングを堆積する。 - 請求項11のプロセスにおいて、
各シャワーヘッド区画を通って供給される蒸気化された前駆体は、同じである。 - 請求項11のプロセスにおいて、
多層基板は、1つ、又はそれ以上のシャワーヘッド区画を通って、異なるタイプの蒸気化された前駆体を、供給することにより製造される。 - 請求項11のプロセスにおいて、
前記蒸気化された前駆体は、YBCO、SmBCO、及び他の希土類混合酸化物から選択されるものである。 - 請求項11のプロセスにおいて、
前記コーティングの全厚さは、1.5ミクロンを超え、
コートされた基板は、少なくとも100アンペア/cm幅の臨界電流を持つ。 - 請求項11のプロセスにおいて、
各コート層の厚みは、1.5ミクロンより大きくない。 - 請求項11のプロセスにより準備される多コートされる基板テープ。
- 請求項17の基板であって、
前記多コート基板は、その上に堆積された、少なくとも2つの異なる組成のコーティングを持つ。 - 請求項17の基板であって、
前記基板は、YBCO、SmBCO、YBCO、SmBCO、及びYBCOの連続的な層がコートされたものである。 - 請求項17の基板であって、
前記コーティングの全厚さは、1.5ミクロンを超え、
コートされた基板は、少なくとも100アンペア/cm幅の臨界電流を持つ。 - 請求項17の基板であって、
各コート層の厚みは、1.5ミクロンより大きくない。 - 多層コートされた基板を製造するMOCVD堆積装置において、
真空チャンバーと、
多ゾーンヒータと、
前記多ゾーンヒータ内のゾーンの数に等しい数の区画を持つ多区画シャワーヘッドと、
前記多区画の各区画に接続された分離された前駆体駆動システムであって、その各々は、液体イットリウムーバリウムー銅前駆体のソースと、ポンプと、不活性ガスソースと、前駆体蒸気化器と、酸素ソースと、
基板移動システムとを備え、
前記シャワーヘッドと前記ヒータとの間の空間は、コーティングの連続的な層が堆積される真空チャンバー内の延長された長さの堆積ゾーンを定義している、
ことを特徴とするMOCVD堆積装置。
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PCT/US2004/016639 WO2005081658A2 (en) | 2003-06-23 | 2004-05-25 | Metalorganic chemical vapor deposition (mocvd) process and apparatus to produce multi-layer high-temperature superconducting (hts) coated tape |
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